Process for after-washing freshly dyed textile material

ABSTRACT

A PROCESS FOR AFTER-WASHING FRESHLY DYED FIBROUS MATERIAL FROM AN ORGANIC MEDIUM, WHEREIN THE FIBROUS MATERIAL IS MOVED ABOUT IN A CHLORINATED ALIPHATIC HYDROCARBON WHICH MAY CONTAIN A TENSIDE AND/OR A DIPOLAR, APROTIC SOLVENT, WITH THE INTRODUCTION OF HEAT, AND THE ORGANIC SOLVENT IS THEM REMOVED.

United States Patent Int. Cl. B08b 3/00; D06f US. (:1; 8-137 12 Claims ABSTRACT OF THE DISCLOSURE A process for after-washing freshly dyed fibrous material from an organic medium, wherein the fibrous mate,- rial is moved about in a chlorinated aliphatic hydrocarbon which may contain a tenside and/or a dipolar, aprotic solvent, with the introduction of heat, and the organic solvent is then removed.

The present invention provides a process for afterwashing freshly dyed fibrous material from an organic medium, wherein the fibre material is moved about in a chlorinated aliphatic hydrocarbon which may contain a,

tenside and/or a dipolar, aprotic solvent, with the introduction of heat, and the organic solvent is then removed.

As substrates there may be used textile materials from synthetic fibres, for example acrylic or acrylonitrile fibres, polyacrylonitrile fibres and copolymers from acrylonitrile and other vinyl compounds, such as acrylic esters, acrylamides, vinylpyridine, vinyl chloride or vinylidene chloride, copolymers from dicyanoethylene and vinyl acetate, as well as acrylonitrile block copolymers, fibres from polyurethanes, metal-modified or basically modified or unmodified polyolefines, especially polypropylene, cellulose triand 21/2-acetate and particularly fibres from polyamides, such as nylon-6, nylon-6,6 or nylon-12, from aromatic polyesters, for example those from terephthalic acid and ethyleneglycol or 1,4-dimethylcyclohexane, and copolymers from terephthalic and isophthalic acid and ethyleneglycol or natural fibres, for example from wool, silk or cotton, as well as regenerated cellulose materials.

Examples of a solvent which must to a great extent be inert towards the fibres or filaments even at dyeing temperature, i.e. must not dissolve the latter, are halogenated aliphatic hydrocarbons, such as carbon tetrachloride, chloroform, methylene chloride, trichloroethylene, tetrachloroethane, dibromoethylene and especially perchloroethylene or trichloroethylene.

The chlorinated hydrocarbons may contain in addition a dipolar, aprotic solvent, such as N,N-dimethylformamide, N,N dimethylacetamide, bis-(dimethylamido)- methane phosphate, tris-(dimethylamido)-ph0sphate, N- methyl-pyrrolidone, 1,5-dimethylpyrrolidone, N,N-dimethyl-methoxy-acetamide, N,N,N',N-tetramethylurea, tetramethylenesulphone (Sulfolan), 3-methylsulfolan or dimethylsulphoxide. Such dipolar solvents preferably have a dipole moment greater than 2.0, especially greater than 3.0.

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In order to avoid damage to the fibres, as a rule more than 50% of the chlorinated aliphatic hydrocarbon is added.

Preferred mixtures contain, for example, 2 to 30% by weight of an aprotic solvent and 98 to by weight of a chlorinated, advantageously aliphatic hydrocarbon.

The present process is advantageously carried out with out the addition of a dispersant. An advantage as a result of this is easier drying of the washed textile'rnate rial by evaporation of the solvent. Tensides may optionally be added to the washing liquor, particularly as additives to hydrophobic solvents with relatively slight dis solving capacity.

Specially important tensides of a suitable nature are the following non-ionic compounds:

(a) Ethers of polyhydroxy compounds, for example, polyoxyalkylated aliphatic alcohols, polyoxyalkylated polyols, polyoxyalkylated mercaptans and aliphatic amines, polyoxyalkylated alkylphenols and alkylnaphthols, polyoxyalkylated alkylarylrnercaptans and alkylaralamines;

(b) Fatty acid esters of the ethyleneglycols and polyethyleneglycols, of propyleneglycol and butyleneglycol, of glycerol, of the polyglycerols and of pentaerythritol, as well as of sugar alcohols, for example, sorbitol, sorbitans and of saccharose;

(c) N hydroxyalkylcarbonamides, polyoxyalkylated carbonamides and sulphonamides.

Examples of tenside in these groups which may be advantageously used are: adducts of 8 mols of ethylene oxide with 1 mol of para-tertiary octylphenol, or of 15 or 16 mols of ethylene oxide with castor oil, or of 20 mols of ethylene oxide with the alcohol C H OH, ethylene oxide adducts with di[a-phenylethyH-phenols, polyethylene oxide-tertiary dodecyl thioether, polyamine-polyglycol ether or adducts of 15 or 30 mols respectively of ethylene oxide with 1 mol of the amine C H NH or C13H3'7NH2.

Especially valuable tensides are sodium sulphosuccinate, sodium alkylaryl sulphonates, amine-.alkylaryl sulphonates, fatty acid esters of sorbitol, ethoxylated alkanolamides, ethoxylated phenols and ethoxylated phosphate esters. The tensides have advantageously H.L.B. values of 3 to 8. The definition of the H.L.B. values can be found in the book Interfacial Phenomena by J. T. Davies and E. K. Rideal, New York, 1963, pp. 371 to 373.

For rinsing, the textile material to be dyed may be in the form of loose material, fleeces, yarn or as knitted goods or fabrics. It is Washed in loose form or in a form put on to a mechanical device in a stationary bath, particularly in a jigger appropriate for this purpose, winch vats or cheese dyeing machines, depending on the ntaure of the goods to be dyed, especially in drum types of washing machines heat having to be applied. The temperature of the washing liquor is advantageously 40 to C;

Rinsing can be carried out in apparatus or vessels which are connected with the external atmosphere (if desired by a reflux condenser) or in closed vessels, such as pressure vessles, with or without pressure.

When rinsing is complete the dyed goods are taken out of the solvent bath and, to remove any solvent still adhering, are treated either with steam or with a hot current of air.

. 3 v 4 The following examples illustrate the invention, the 100 parts of dry, unpre-treated polyacrylonitrile parts and percentages being by weight unless otherwise knitted goods (Orion high bulk) were added and dyed at stated. a goods-to-liquor ratio of 1:40 for 45 minutes at boiling EXAMPLE 1 temperature (121 C.) in a flask equipped with a refluX 0. art of the d e t 1, -dih drox -4,8-diamino-3,7- 5 9 with P F P 9 g f g g fi i boiling tempera mg to the d1st1llat1on+refiux principle) with the addltlon ture in perchloroethylene and the solution then cooled to of 1 Part of the product of the formula about 100 C. 2.5 parts of unpre-treated textured polyester knitted goods (Crimplene) were added to the solution and in 100 parts of perchloroethylene at a goods-to-liquor 10 CH3 CH3 ratio of 1:64 were dyed for 45 minutes at boiling temperature (121.2 C.) in a boiler equipped with a reflux cooler with recovery of the evaporating solvent. The batch was then cooled for minutes and the dyed yarn freed from the adhering dye liquor by centritugation. Without any 15 intermediate drying, the unfixed dyestutf adhering to the surface was removed by an after-treatment for 5 minutes The batch was then cooled for 15 minutes and the dyed at 50-60" C. in perchloroethylene in order to obtain the knitted goods free from any adhering dye-liquor by centrifdesired brilliant tints an the maximum fastness properties. ugation.

The batch was then centrifuged and dried in a warm cur- Without any intermediate drying, the unfixed dyerent of air. stufl' adhering to the surface was removed by brief The effect obtained with this after-treatment (purity of rinsing with cold perchlorethylene containing 10% ditint, fastness properties) corresponds to that of a similar methylacetamide, and subsequent treatment in the same dyeing that can be obtained subsequent to dyeing with a solvent mixture but with the addition of 2 g./l. of the blank vat consisting of 5 m1./ 1. NaOH 10 n. and 2 g./l. oleic acid ester of polyethyleneglycol 3-00 at 40 C. for

hydrosulphite by treatment from an aqueous solution for about 10 minutes in order to obtain the desired brilliant minutes at 60 C. tint and the maximum fastness properties. The dyeing EXAMPLE 2 was then centrifuged directly after leaving the bath, and

dried.

A red dyeing prepared by the exhaust process on nylon- 30 By this after treatment the same efiect is obtained as '6'tuftmg carpet (Peflon) wlth the dyestufi of the formula when the dyeing is after-cleaned by hot treatment in C1 water with 2 g./l. of an adduct of 1 mol of nonyl- O O phenol and 9 mols of ethylene oxide. voi-omorti-rniso N=N N(GHzCHzQH)z EXAMPLE 4 was freed from the adhering dyeliquor by centrifugation was dissolved in 10 parts by volume of hot water. The subsequent to dyeing. Without any intermediate drying, 59 solution was cooled and treated with calcined sodium the unfixed dyestuff adhering to the surface was removed carbonate up to a concentration of 10 g./l. The resultby washing with cold perchloroethylene for 5 minutes and ing dyestuif solution was mixed with 90 parts by volume a then treating for about 10 minutes with a perchloroof perchloroethylene containing 20 g./l. of an oleic acid ethylene dyeliquor at 4050 C. which contains 2 g./l. ethylene oxide adduct (average molecular weight 300 polyethyleneglycol-(300)-oleic acid ester, in order to ob- To the emulsion so prepared there were added 10 parts 'tain the desired brilliant tints and the maximum fastness of dry unpre-treated mercerised cotton yarn. Dyeing was properties. carried out without any further additions at a goods-to- Subsequent to this treatment to batch was again rinsed liquor ratio f 1:3 (10 pal-ts f yarn in 200 parts by briefly with cold perchloroethylene, then centrifuged and volume of dyebath; density of the 61) after dried. The effect obtained with this after-treatment corheating for 45 minutes at boiling temperature in an responds to that of a similar dyeing which is produced with Open system with recovery of the evaporating Solvent a conventional detergent from a hot aqueous dyeliquor. by means of a reflux condenser The cotton yam was EXAMPLE 3 then freed from the dyeliquor still adhering by cen 2 parts of the dyestufl of the formula 65 mfueatlon- 7 H0 N CH3 Without any intermediate drying the dyestufl'f not rem actively fixed was removed by brief rinsmg with per- N= O' Z1161 chloroethylene and subsequent treatment for about 10 N minutes at 5060 C. with a perchloroethylene and water emulsion (9:1) containing 10 g./l. of the oleic in the form of a concentrated dyestuff powder were disflcid fistel' 0f p ly thyeneglycol (molecular weight 300-) solved at boiling temperature in a solvent mixture conorder to obtam the f bnnlant {mt f the maxi sisting of parts of perchloroethylene and 5 parts of mum fastlless P P 'sllbseflllellt to 1111s treatment dimethylacetamide, and the solution then cooled to about the batch was briefly Imsed Wlth Cold p y C 75 one, the goods then centrifuged and dried.

The effect obtained with this after-treatment corresponds to that of an ordinary after-treatment from a boiling aqueous liquor with the addition of a synthetic detergent or soap.

EXAMPLE Polyester filament fabric (Terylene twill) was padded with a solution consisting of 20 parts of the dyestuif of the formula I C2H4OCOCH in 1000 parts of a mixture of 90% perchloroethylene and dimethylacetamide in the cold, squeezed to a weight increase of 34% referred to the weight of the fibre, dried at 4050 C. in a warm current of air and then thermoset for 60 seconds at 210 C. The fabric was then after-cleaned by continuous treatment on a wide installation for after-treatment, first in a mixture of cold perchlorethylene and dimethylacetamide (9:1) (2 passages) and then hot treatment at 40-50 C. with 2 g./l. of the oleic acid ester of polyethyleneglycol 300 (1-3 passages) in the same solvent mixture, and by brief cold rinsing finally (1-2 passages) with pure perchloroethylene. The goods were then squeezed on a mangle and dried. By this after-treatment from a solvent a brilliant red dyeing fast to rubbing was obtained.

EXAMPLE 6 A nylon-6,6 fabric was paddes with a solution consisting of 10 parts of the dyestuif of the formula al lNa aMQ 1000 parts of a mixture of 90% perchlorethylene and 10% dimethylacetamide in the cold, squeezed to a weight increase of 42% referred to the weight of the fibre, dried at 4050 C. in a warm current of air and then thermoset for 1 minute at 200 C. The fabric was then after-cleaned by continuous treatment on a wide after-treatment installation, first by cold rinsing (1-2 passages) with pure perchloroethylene, then passing it through 1 to 3 warm baths (50 C.) of perchloroethylene which contains 3 g./l. of cleansing intensifier, and brief rinsing with cold perchlorethylene (l passage).

By this after-cleansing from the solvent the dyestuff not reactively bound is peeled off the fibre and a brilliant yellow dyeing obtained which is fast to rubbing and wetting.

EXAMPLE 7 Polyacrylonitrile staple fabric (Orlon) was padded with a solution consisting of 10 parts of the dyestufi of the formula (H) IIIHOH;

g I l H (CH2) 3N (CH3) 2 in 1000 parts of perchlorethylene in the cold and squeezed to a weight increase of 106% referred to the weight of the fibre. The fabric was dried and then thermoset for 90 seconds at 200 C. Subsequent to the thermosetting the fabric was after-cleansed by continuous treatment on a wide after-treatment installation by brief rinsing (l passage) in perchlorethylene at 60 C. and then by being passed through 1 to 2 baths of cold perchlorethylene which contained 2 g./l. of the oleic acid ester of polyethyleneglycol 200, and brief rinsing (1 passage) with warm perchlorethylene at 40 C. By the after-treatment with a solvent there is obtained a blue dyeing which is more even and fast to rubbing than a dyeing has not been after-treated.

EXAMPLE 8 A dyeing, prepared in the continuous dyeing process according to the thermosetting method (2 passages through the padder in the cold, drying for 1 minute at C., thermosetting for 2 minutes at 140 C.) with 10 g./l. of the dyestuif of the formula OCHa G1 and pure perchlorethylene as solvent on a non-modified polypropylene fabric, was after-cleansed after the thermosetting by continuous treatment on a wide after-treatment installation by rinsing with perchlorethylene at 60 C. (1 passage) and then rinsing with warm perchlorethylene at 40 C. which contains 2 g./l. of the oleic acid ester of polyethyleneglycol 300.

Finally, the batch was rinsed again by being passed through cold perchlorethylene, squeezed and dried.

A dyeing purer and faster to rubbing was obtained by applying the after-treatment with a solvent, in comparison with an untreated dyeing.

EXAMPLE 9 A bleached woolen fabric was padded with a cold solution (10 g./l.) of the dyestuff of the formula in a mixture of perchlorethylene and dimethylacetamide (9:1) in two passages, dried at 100 C. for a 1 minute and thermoset for 1 minute at 200 C. The dyed woolen fabric was after-cleansed subsequent to the thermosetting by continuous treatment at boiling temperature on a wide after-treatment installation (2-4 passages) with perchlorethylene which contains 5 g./l. of an adduct from octadecyl alcohol and 35 mols of ethylene oxide. After this after-treatment with the solvent, the batch was rinsed with cold perchlorethylene once, squeezed and dried.

A brilliant and fast yellow dyeing was obtained. The tint and fastness properties of this dyeing correspond to those which are obtained by an ordinary aqueous hot rinsing with the addition of synthetic detergents.

We claim:

1. A process for after-washing textile materials freshly dyed from an organic medium which comprises agitating said textile material in a liquid medium comprising a chlorinated hydrocarbon inert toward textile material at a temperature of from 40 to C. and thereafter removing said liquid.

2. A process as claimed in claim 1, wherein only fully synthetic fibres prepared by polymerisation or polycondensation are used.

3. A process as claimed in claim 1, wherein textiles consisting at least partially of natural fibres are used.

4. A process as claimed in claim 1, wherein washing is carried out continuously in connection with a continuous dyeing process.

5. A process according to claim 1 in which the afterwashing medium contains a non-ionic tenside, a dipolar aprotic solvent having a dipole moment greater than 2.0 or a mixture thereof, said dipolar aprotic solvent being selected from N,N-dimethylformamide, N,N-dimethylacetamide, bis-(dimethylamido)-methane phosphate, tris- (dimethylamido)-phosphate, N-methyl-pyrrolidone, 1,5- dimethyl-pyrrolidone, N,N-dimethyl-methoxy-acetamide, N, N, N, N tetramethylurea, tetramethylene sulphono (Sulfolan), 3-methylsulfolan or dimethylsulphoxide.

6. A process according to claim 1 wherein an emulsion of 90% chlorinated hydrocarbon and 10% water is used.

7. A process as claimed in claim 3, wherein woolen textile materials are used.

8. A process as claimed in claim 3, wherein cotton textile materials are used.

9. A process as claimed in claim 3, wherein union fabrics of natural and synthetic fibers are used.

10. A process as claimed in claim 5, Where the dipolar solvent is N,N-dimethylformamide or N,N-dimetlrylacetamide.

References Cited UNITED STATES PATENTS 3,290,111 12/ 1966 Hees et al. 8-165 MAYER WEINBLATI, Primary Examiner US. Cl. X.R. 

